Method and emans for preparing explosives, and resulting explosives



Patented Mar. 26, i

i v UNITED 1 STATES R 1,706,871 PATENT OFFICE;

HERBERT caveman, or nrcrmonn, NEW YORK.

METHOD AND MEANS FOR PREPARING EXPLOSIVES, AND RESULTING EXPLOSIVES.

80 Drawing.. Application filed May 2, 1925, Serial No. 27,845; Renewed August 7,1928.

My. present invention relates to methods of fabricatin absorbents for liquid oxygen for use as explosives, and particularly to carbonaceous absorbents derived from the lignin 5 liquors or residues obtained in the manufacture of wood pulp vby the alkali (soda) or other suitable process, but particularly by the alkali (soda) process, and aims to devise methods of the general character speci- 10. fied which are simple to practice, easy, economical and convenient to carry out, requiring simple apparatus and few manipulations for this purpose, and which result in a superiorproduct for the intended purpose, thls product, which also comprisesa part of the present invention, being characterized by its high density, its high degree of absorptivene ss for liquid oxygen, its high degree of retentiveness for the absorbed liquid oxygen, and its high degree of combustibility, all desirable properties for the intended purpose.

My invention includes also the resulting explosive and cartridge containing the same, and involves other advantages in manipulation, use and superiorities of the process and resulting product which will in part be point-- ed out hereinafter and which will in part-be obvious to those skilled in the art to which the'present invention relates. V

In the accompanying specification I shall describe an illustrative embodiment of the method of the present invention. In the acproducts may be made by other embodiments of the process than that herein specifically described for purposes of example merely.

Referring tothe aforesaid illustrative embodi-ments of the present invention, and particularly to the aforesaid illustrative embodi ment of the method, I' prefer to use as the raw material for the fabrication of the product of the present invention liquors rich in dissolved lignin, preferably such liquors de way of illustration merely, and that the rived from the manufacture of wood pulp .by the alkali (soda) process, especially where wood pul is derived from woods, such as spruce, pme'and the like, rich in resins or other forms of lignin. Such liquors areparticularly desirable, since they yield a high purity carbon characterized by high density and great absorptiveness and retentiveness for liquid oxygen, as hereinafter described in considerable detail. I These liquors are now carbonized, preferably with controlled access of air or even with the total exclusion of air. This is done in order to prevent too great combustion and consequent loss of carbon values in the final material. Preferably such carbonization takes place in retorts which are sealed against the ingress of air or to which air is admitted in very small amounts only to carry off by combustion or otherwise more volatile carbonaceous materials to thus leave a very open or porous carbonized lignin residue in the retort.

The carbonized lignin residues thus obtained will be found to be in a granular condition, the grains of which vary in size to a considerable degree andare quite uneven The material also will be found to contain in the pores thereofa considerable amount, often as high as ten (10) per cent, of. alkaline carbonates, particularly sodium carbonate, where the pulp has been made by the soda process, together with other mineral substances. The carbonized lignin residues thus obtained are now thoroughly leached, first with water, to remove water-soluble mineral substances, and thereafter, if desired, although this step may be omitted, with acidulated water, such as water acidulated with about one-half to one per cent of hydrochloric acid, toremove acid-soluble mineral' 'substances. The purpose of this treatment or treatments is to reduce to a minimum the mineral constitutents of the carbon so as to obtain a carbon characterized by maximum combustibility.

I now take the leached carbonized lignin residues, whether or not the same-have been previously subjected to the acid treatment specified above, and submit the same to a slight grinding action to reduce the grains to a more or less uniform size so that the largest grains are not more than about one-quarter of an inch in their longest dimension and so that not more than about twenty five percent 11 of the material wi ass through a one hun dred mesh screen. I (hire should be taken duringthis slight grinding action, the purpose of which is to obtain a moreuniform, evensized material which isvery suitable for use in smaller sized cartridges, to see that the material isnot too finely round, which would convert it from a hig ly absorptive a container as it woul be into the cartridge and to take care of any liquid oxygen thatwrapper, should be not less than about 0.20. I have also found that the degree of absorptiveness of the material for'liquid oxygen should be not less than about 2.6 times its own weight, and preferably about 3.0 times its own welght, or even over, so as to be suitable for use under actual field conditions mightbe evaporated up to the time that the cartridge is actually exploded.

It may here be stated, that by carefully controlling the carbonization of the lignin liquors or residues in the retorts, grains of the proper size may be and often are obtained without any. grinding action whatsoever. In any event, the grinding action should be carefully controlled and regulated to yield a carbon characterized .by a high degree of absorptiveness and a comparatively low degree of decolorizing power, rather than a low degree of absorptiveness and a high degree of decolorizi'ng power. I have found that the properties of absorptiveness and decolorizing power vary generally in approximately inverse proportion, absorptiveness depending on a comparatively large grain and being characterized by a comparatively low degree of decolorizing power, decolorizing power being apparently dependent upon small grains of a low degree of absorptiveness.

The material obtained as above described may now be packed into suitable cartridge containers, I prefer to use a containerv which is completely and readily combustible and which has proper insulating properties to prevent too ready absorption of heat with conse uent evaporation of the liquid oxygen. For t llS purpose I prefer to use a cartridge container which has a cotton fibre base, such as certain red fibre papers which may be readily obtained in the open market. This paper may readily be formed into containers of the desired size which are then, packed with the granular leached. carbonized lignin residues obtained asabove described, after which the liquid oxygen is added, the caroured as freely into .tridge sealed, stored and finally put i'n' place, and exploded by a'percussion cap or other The material obtained as above describedis characterized by its high density, its uni-. formity, its high degree of absorptiveness and its correspondingly high degree of retentiveness for the liquid oxygen, making it ple to practice, makesuse of an otherwise waste material, and requires very simple apparatus and few manipulations for its successful practice. The absorbent itself sesses the many advantages already spec fied above, and the resulting explosive and car-' tridges containing the same are further characterized by their cheapness, the ease with which they may be prepared. and their remarkable efliciency in use under actual field conditions. Other advantages of the present invention will readily occur to those skilled in the art .to which the same relates.

What I claim as my invention is:

1. The method of preparing'granular carbonized lignin residues for use as an absorbent for liquid oxygen, which comprises leaching said material to substantial freedom from water-soluble mineral matters to reduce the proportion of incombustible constituents of said material to a minimum and reducing the grains of the carbonized mate rial to such a size that their density will be at least equal to about 0.20 and their degree of absorptiveness for liquid oxygen at least equal to 2.6 times their own weight.

2. The method of preparing granular carbonized lignin residues for use as an absorbent for liquid oxygen, which comprises leaching said material with an acid solution to substantial freedomfrom water-soluble and acid-soluble mineral matters to reduce the proportion of incombustible constituents of said material to a minimum and reducing thegrains of the carbonized material-to'such a size that their density will be at least ual to about 0.20 and their degree of absorptiveness for liquid oxygen at least equal to 2.6 times their own weight.

3. The method of preparing granular carbonized lignin residues for use as an absorbent for liquid oxygen, which comprises leaching said material to substantial free-.

dom' from water-soluble mineral matters to reduce the proportion of incombustible constituents of said material to a minimum'and reducing the grains of the carbonized material to such a size that their density will be at least equal to about 0.20 and their degree of absorptiveness for liquid oxygen at least equal to 3.0 times their own weight.

w 4. The method of preparing granular carbonized lignin residues for use as an absorbent for liquid .ox gen, wh ichcom r ses leaching said material with an acid so ut on to substantial freedom from water-soluble and acid-soluble mineral matters to reduce the proportion ofincombustible constituents of said material to a minimumand reducing the grains of the carbonized material to such a size that their density will be at least equal to about 0.20 and their degree of absorptiveness for liquid oxygen at least equal to 3.0

' timestheir own weight.

' 5. The method of preparing granular carbonized lignin residues for use as an absorbent for liquid oxygen, which comprises leaching said material with an acid solution to substantial freedom from water-soluble and acid-soluble mineral matters to reduce the proportion of fincombustible constituents of said material to a minimum and reducing the grains of the carbonized material to such a size that not more-than twenty-five (25) per. cent of the material will pass through a onehundred mesh screen and their density will beat least equal to about 0.20 and their degree of absorptiveness for liquid oxygen at least equal to 3.0 times their own weight.

6. The method of preparing granular carbonized lignin residues for use as an absorbent for liquid oxygen, which comprises leaching said material with an acid solution to substantial freedom from water soluble and acid-soluble mineral matters -to reduce the proportion of incombustible constituents of said material to a minimum and reducing the grains of the carbonized material to such 40 a size that not more than twenty-five (25) per cent of the material will pass through a one hundred mesh screen and their density will be at least equal to about 0.20 and their degree of absorptiveness for liquid oxygen at least equal to 2.6 times their own weight.

7. The method of preparing granular carbonized lignin residues for use as an absorbent for liquid oxygen, which comprises leaching said material to substantial freev5o dom from water soluble mineral matters to ,reduce the proportion of incombustible constituents of said material to a minimum and reducing the'grains of-the carbonized mate rial to such a size that not more than twentyfive (25) per cent of the material will pass through a one hundred mesh screen and their density will be at least equal to about 0.20 and their degree of absorptiveness for liquid oxygen at least equal, to, 3.0 times their own weight.

8. The method of preparing granular car- 5 bonized lignin residues for use as an absorbent for liquid oxygen, which comprises leaching said material to substantial free- I dom from water-soluble mineral matters to reduce the proportion of incombustible constituents of said material to a minimum and reducing the grains of the carbonized mate) rial to such a size that not more than twentyfive (25) per cent of the material will pass through a one hundred mesh screcnand their density will be at least equal to about 0.20 and their degree of absorptiveness for liquid oxygen at least equal to 2.6 times their own weight.

9. The method of preparing carbonaceous material for use as an absorbent for liquid oxygen for use as ancxplosive, which comprises, carbonizmg liquors rich in dissolved lignin material with controlled access of airto form a granular carbonized lignin re sidue, and thereafter leaching said material with an acid solution to substantial freedom from water-soluble and acid-soluble mineral matters to reduce the proportion of incombustible constitutentsof said material to a minimum and reducing the grains of the carbonized material to-such a size that their density will be at least equal to about 0.20 and their degree of absorptiveness'for liquid oxygen at least equal to 3.0 times their own weight.

10. The -method of preparing carbonaceous material for use as an absorbent for liquid oxygen for use as an explosive, which comprises. carbonizing liquors rich in dissolved lignin material with controlled access of air to form a granular carbonized lignin residue, and thereafter leaching said material with an acid solution to substantial. freedom from water-soluble and acid-soluble mineral matters to reduce the proportion ofincombustible. constitutents of said ma-. terial to a minimum and reducing the grains of the carbonized material to such a size that their density will be at least equal to about 0.20 and their degree of absorptiveness for liquid ,oxygen'at least equal. to 2.6 times their own weight.

11. The 'rnethodof preparing carbonaceous material for use as an absorbent for liquid oxygen for use as an explosive, which comprises carbonizing liquors rich in disv solved lignin material with controlled access of air toform a granular carbonized lignin residue, and thereafter leaching said material to substantial freedom from watersoluble mineral matters to reduce the pro.- portion of incombustible constituents of said material to'a mini-mum and reducing 120 the grains of the carbonized material to such a size that their density will be at. least equal to about 0.20 and their degree of ab-' sorptiveness for liquid oxygen at least equal to 3.0 times their own weight.

12. The method of preparing carbonaceous material for use .as an absorbent for liquid oxygen for use as an explosive, which comprises carboniz-ing liquors rich in dissolved lignin material with controlled access of air to form a granular carbonized lignin residue, and thereafter leaching said'material twsribstaiitial freedom from watersoluble mineral matters to reduce the proportion of incombustible constituents of said material to a minimum and reducing the grains of the carbonized material to such a size that, their density will be at least 'equal to about 0.20 and their degree of absorptiveness for liquid oxygen at least equal to 2.6 times their own weight.

13. An absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble mineral matters and having a minimum proportion of incombustible constituents, the density of the material being at least equal to about 0.20 and the degree of absorptiveness of the material for liquid oxygen being at least equal t0'2.6 times its own weight.

14. An absorbent, for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble and acid-soluble mineral matters and having a minimum proportion of incombustible constituents, the density of the material being at least equal to about 0.20 and the degree of absorptiveness of the material for liquid oxygen being at least equal to 2.6 times its own weight. w

15. An absorbent for liquid oxygen. for use as an explosive,-' comprising granular carbonized lignin residues substantially free from water-soluble mineral matters and having a minimum proportion of incombustible constituents, the density of the material being at least e ual to about 0.20 and the'degree of absorptlveness of the material for liquid oxygen being at least equal to 3.0 times its own Weight.

16. An absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble and acid-soluble mineral matters and having a minimum proportion of incombustible constituents, the density of the material being at least equal to about 0.20 and the degree of absorptiveness of the material for liquid oxygen being at least equal to 3.0 times its own weight.

17. An absorbent for liquidoxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from Water-soluble and acid-soluble mineral matters and having a minimum proportion of incombustible constituents, the grains of the material being of such a size that not more than twenty-five (25) per cent of the material will pass through a one hundred mesh screen.

18. An absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble mineral matters and having a minimum proportion of incombustible contituents, the grains ofv the material being of such a size that not more than the material being at least equal to about 0.20 and the degree of absorptiveness of the material for liquid oxygen being at least carbonized lignin residues substantially free from water-soluble and acid-soluble mineral matters and having a minimum proportion of incombustible constituents, the density of i equal to 2.6 times its own weight, the grains Q the material being of such a size that not more than twenty-five (25) per cent-of the material will pass through a one hundred.

mesh screen. v

20. An absorbent for liquid oxygen for use as an explosive, comprising granular -carbonized lignin residues substantially free from water-soluble mineral matters and having a mmlmum proportlon of lncombustible constituents, the density of the material being at least equal to about 0.20 and the degree of absorptiveness'of the material for liquid oxygen being at least equal .to 2.6 times its own weight, the grains of the material being of such a size that not more than twenty-five (25) per cent of the material will pass through a one hundred mesh' screen.

21. A cartridge comprising a combustible container charged with an explosive comprising an absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble and acid-soluble mineral matters and having a minimum proportion of incombustible constituents, the density of the material being at least equal to about 0.20 and the degree of absorptiveness of the material for liquid oxygen being at least equal to 2.6 times its own weight, the grains 0 the material being of such-a size that not more than twenty-five '(25) per cent of the material will pass through aone hundred mesh screen, said absorbent containing absorbed therein an amount of liquid oxygen.

sufiicient for complete combustion of the absorbent under actual field conditions and allowing for average evaporation of liquid oxygen.

22. A'cartridge comprising a combustible container charged with an explosive comprising an absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free.

mesh screen, said absorbent containing ab- .sorbed therein an amount of liquid oxygen sufiicient for complete combustion of the absorbent under actual field conditions and allowing for average evaporation of liquid oxygen. 4

23, A cartridge comprising a combustible container charged with an explosive comprising an absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble mineral matters and having a minimum proportion of incombustible constituents, the density of the material being at least equal to about 0.20 and the degree of absorptiveness of the material for liquid oxygen being at least equal to 3.0

times its own weight, said absorbent containing absorbed therein an amount of liquid oxygen suflicient for complete combustion of the "absorbent under actual field conditions and allowing for average evaporation of liquid oxygen.

24. A-cartridge comprising a combustible container charged with an explosive eom-. prising an absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble mineral matters and having a minimum proportion of incombustible constituents, the density of the material be ing at least equal to about 0.20 and the degree of absor'ptiveness of the material for liquid oxygen being at least equal to 2.6 times its own weight, said absorbent containing absorbed therein an amount of liquid oxygen suflicient for complete combustion of the absorbent under actual field conditions and allowing for average evaporation of liquid oxygen.

25. A cartridge comprising a combustible container charged with an explosive comprising an absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble mineral matters and having a'minimum proportion of incombustible constituents, said absorbent containing absorbed therein an amount of liquid oxygen suflicient for complete combustion of the absorbent .under actual field .eonditions and allowing foraverage evaporation of liquid oxygen.

26. A cartridge comprising a combustible container charged with an explosive comprising an absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble mineral matters and having a minimum proportion of incombustible constituents, the density of the material being at least equal to about 0.20 and the degree of absorptiveness of the material for liquid oxygen being-at least equal to 2.6 times its own weight, the grains of the material being of such a size that not more than twenty-five (25) per cent of the a material will pass through a one hundred mesh screen, said absorbent containing absorbed therein an amount of liquid oxygen sufiieient for complete combustion of the absorbent under actual field conditions and allowing ,for average evaporation of liquid oxygen.

27. A cartridge comprising a combustible container charged with an explosive comprising an absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble mineral matters and having a minimum proportion of incombustible constituents, the grains of the material being of such size that not more than twenty-five (25) per cent of the material will pass through a one hundred mesh screen, saidabsorbent containing absorbed therein an amount of liquid oxygen sufficient for complete combustion of the absorbent under actual field conditions and allowing foraverage evaporation of liquid oxgen.

28. A cartridge comprising a combustible ,container charged with an explosive compris-- ingan absorbent for liquid oxygen for use as an explosive, comprising granular carbonized lignin residues substantially free from water-soluble and acidsoluble mineral matters and having a minimum proportion of ingombustible constituents, the density of the material being at least equal to about 0.20 and the degree of absorptiveness of the material for liquid oxygen being at least equal to 3.0 times its own weight, said absorbent containing absorbed therein an amount of liquid oxygen sufiicient for complete combustion of the absorbent under actual field conditions and allowing for average evaposorbent containing absorbed therein an amount of liquidoxygen sufiicient for complete combustion of the absorbent underactual field conditions and allowing for average evaporation of liquid oxygen.

30. A cartridge comprising a combustible container charged with an explosive comprising an absorbent for liquid oxygen for 'carbonized lignin residues substantial from yvstemsoluble and acid soluble mineral mntters and having a minimum roportion a of incombustible constituents, sa'" absorbent containing absorbed therein an amo unt of liquid oxygen sufiicient for complete com- April, 1925.

bastion. of the absorbent linden actnsl field 'oonditions and allowing for average evaporation of liquid ox gen. In testimony, w 'ereof, I have. signed my name to this 'speoifieation this 8th day of HERBERT GBUGBIRD. 

